GladiATRTM Vision Single Reflection ATR Accessory

Installation and User Guide

The information in this publication is provided for reference only. All information contained in this publication is believed to be correct and complete. PIKE Technologies, Inc. shall not be liable for errors contained herein nor for incidental or consequential damages in connection with the furnishing, performance, or use of this material. All product specifications, as well as the information contained in this publication, are subject to change without notice. This publication may contain or reference information and products protected by copyrights or patents and does not convey any license under the patent rights of PIKE Technologies, Inc. nor the rights of others. PIKE Technologies, Inc. does not assume any liability arising out of any infringements of patents or other rights of third parties. This document contains confidential or proprietary information of PIKE Technologies, Inc. Neither this document nor the information herein is to be reproduced, distributed, used or disclosed, either in whole or in part, except as specifically authorized by PIKE Technologies, Inc. PIKE Technologies, Inc. makes no warranty of any kind with regard to this material including, but not limited to, the implied warranties of merchantability and fitness for a particular purpose. Copyright 1991-2015 by PIKE Technologies, Inc., Madison, WI 53719. Printed in the United States of America. All world rights reserved. No part of this publication may be stored in a retrieval system, transmitted, or reproduced in any way, including but not limited to, photocopy, photograph, magnetic or other record, without the prior written permission of PIKE Technologies, Inc. Address Comments to: PIKE Technologies, Inc. 6125 Cottonwood Drive Madison, WI 53719 Phone (608) 274-2721 Fax (608) 274-0103 E-mail info@piketech.com Web Site www.piketech.com Jan. 1, 2015

Contents

Introduction 1 GladiATR Assembly View 2 Unpacking Your Accessory 3 Packing List 3 Assembly 5 Installation 7 Accessory Installation 7 Software Installation 8

Installing Videology Image Capture Software 8 Interfacing the GladiATR Vision 8

Installing IC 2.2 Image Capturing Software (BNC) 9 Accessory Alignment 10 Adjusting Camera Focus 11 Performance Verification 12 Sampling Procedures 13 Sample Analysis with High-Pressure Clamp 14 Pressure Clamp Tip Attachments 15 Configuration for Liquid Sampling 16

Configuration for Solid Sampling 18 Configuration for Powder Sampling 19 Crystal Cleaning 19 Effects of Temperature 19 ATR Spectra 20 ATR Correction 21 Useful Equations 22 Solid Samples 22 Crystal ATR Materials 22

Diamond 22 Germanium 22

Precautions 23 Mirrors 23 SAFETY 23 Environmental Ratings 24 Specifications 24 Power Supply Symbol Definitions 25 Replacement Parts and Options 26

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Introduction

GladiATR Vision – Diamond ATR with Sample View The GladiATR Vision™ is a novel sampling tool which couples small area infrared analysis with simultaneous viewing. Samples are placed face down and positioned on the diamond crystal while its image is projected in real-time on the LCD screen. Finding and optimizing the sample placement for specific analysis areas is easy and fast. Analysis of thick or non-transparent samples is no problem because viewing is through the diamond crystal.

The GladiATR Vision accessory utilizes an innovative optical design with IR beam and visible optical image converging at the sample position – ensuring that “What you see is what you sample!” The 110X magnification of the sample image enables the positioning of even relatively small samples into the center of the diamond crystal for optimized analysis. Analysis of samples as small as 50 microns in size is possible with the GladiATR Vision accessory.

The GladiATR Vision optical design is all reflective, preserving the full spectral range inherent to diamond. For standard mid-IR FTIR spectrometers, the spectral range available with the GladiATR Vision will be 4000 – 400 cm-1. For FTIR spectrometers equipped with far-IR optics, the spectral range is extended to less than 50 cm-1.

Utilizing the diamond crystal of the GladiATR Vision with its 45° angle of incidence the depth of penetration of the IR beam for most organic samples is about 2 microns at 1000 cm-1. This small depth of penetration enables most liquid, solid, polymer, gels or paste samples to be measured without any sample preparation – greatly saving analysis time compared to conventional transmission sampling techniques. Solid samples are placed upon the diamond ATR crystal, pressure is applied via the click-stop pressure clamp and the spectrum is collected. Liquid samples are simply applied to the ATR crystal and the spectrum is collected. If the liquid sample is volatile the optional Liquids Retainer should be attached to the crystal plate and the Volatiles Cover is placed over the sample before the spectrum is collected.

Options for the GladiATR Vision include a Ge crystal plate (non-viewing) for high refractive index samples, a specular reflectance plate (non-viewing) for reflectance analysis of coatings on reflective substrates and a Flow-Through Attachment.

The GladiATR Vision offers optional resistively heated crystal plates with maximum temperature operation to 210 °C (diamond) and 130 °C (germanium, non-viewing.) These heated crystal plates are operated via PIKE Technologies temperature controllers – digital/PC or digital versions.

The GladiATR Vision is available in configurations to fit most FTIR spectrometers.

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Figure 1. Assembly view of the GladiATR Vision ATR accessory

NOTE: High-Pressure Clamp, Liquids Retainer and Volatiles Cover are optional and need to be ordered separately.

or USB

High-Pressure Clamp (Optional)

ATR Crystal

ATR Crystal Plate

GladiATR Vision Base Optics

Baseplate Fastener Screw

LCD, On/Off Analog Video Output or USB Power Input, 12V DC

Brightness, Higher/Lower

Purge Inlet

Front Panel (remove to access alignment screws)

Stainless Steel

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Unpacking Your Accessory

In order for you to quickly verify receipt of your accessory, we have included a packing list. Please inspect the package carefully. Contact PIKE immediately if any discrepancies are found. Packing List GladiATR Vision Manual GladiATR Vision Base Unit with

LCD Power Cord GladiATR Top Plate

PN 350-026019 PN 026-19XX PN 026-2004/5 or 6 Quantity 1 Quantity 1 Must Select

GladiATR High-Pressure Clamp Pressure Tips Foam Gaskets PN 026-3020 PN 025-3099 For Purge Tubes Optional One set Quantity 4

Purge Tubing Kit Hex Wrenches Liquids Retainer and Volatiles Cover

PN 025-3055 One set PN 026-5013

Quantity 1 Optional

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Packing List (Continued)

GladiATR Vision Crystal Plate Options

Description Part Number

Diamond Vision Crystal Plate 026-2102

Ge Crystal Plate (non-viewing) 026-2050

Specular Reflection Plate (non-viewing) 026-2200

Specular Reflection Plate (viewing) 026-2202

Heated Diamond Crystal Plate, 210 °C, Vision 026-4101

Heated Ge Crystal Plate, 130 °C (non-viewing) 026-4050

The GladiATR base optics assembly has a crystal plate and the purge tubes attached. Some base optics assemblies may appear different due to specific baseplate mountings for your FTIR. The pressure clamp, pressure tips, purge tubing kit and wrench set are packed separately in the carrying case. The purge tubing kit is not needed with most FTIR models. The swivel tip is attached to the pressure clamp assembly.

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Assembly 1. Attach the GladiATR base optics to its baseplate. This is done by securing the optics base with two

screws, one on each side (Figure2).

Figure 2. Location of screws securing the optics base

2. Install the ATR crystal plate. For proper orientation the serial number is situated at the 1 o’clock position (Figure 3). The support bar is not visible when using the Ge ATR plate. Installing the ATR crystal plate improperly will result in no or very low throughput energy through the accessory.

When installing the 210 °C heated diamond plate and the heated Ge plate align the electrical pins on the plate to the connector pad located on the top of the base optics and continue to follow the instructions for the standard diamond plate described in step 2.

Serial number at 1 o’clock position

Front of accessory

Figure 3. Top view of crystal plate properly seated on the accessory

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3. Place the clamp over the dowel pins located on the top of the accessory. Secure using the two large hex nuts (Figure 4). Instructions for clamp operation are detailed on page 14 of this manual.

4. Complete accessory assembly by pressing the stainless steel top plate over the crystal ATR plate (Figure 5).

Figure 4. Proper placement of clamp on the Figure 5. Proper placement of top plate over top of the accessory the crystal ATR plate

5. If purging is required, press the blue tubing included with the GladiATR into the quick-disconnect

port located on the front of the base optics. To remove the tubing, press the black ring of the opening in and pull the tubing out.

6. For heated configurations, connect the heater cable between the connector (located on the lower left side of the front panel) and the temperature controller.

7. Connect the video power cable to the right lower front of the base optics.

8. Connect the USB or BNC cable, if the BNC video capture option was purchased, to the lower right front of the base optics and to the computer (USB version) or frame grabber box (BNC version).

Hex Nut Hex Nut Stainless Steel Top Plate

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Installation

The GladiATR Vision accessory has been aligned and tested in the PIKE Technologies facility on your model FTIR spectrometer to ensure that it performs to specifications. However, some variation in optical alignment can occur from spectrometer to spectrometer. To allow for this difference, there are adjustable alignment screws within the GladiATR Vision base optics assembly for fine-tuning once the accessory is installed in the spectrometer. The following is the procedure for accessory installation and final alignment.

Accessory Installation 1. Set your FTIR spectrometer to collect data at 4 cm-1 spectral resolution (including the FTIR J-stop). 2. The GladiATR Vision accessory fits into the sample compartment of the FTIR spectrometer. Your

GladiATR Vision is provided with the appropriate sample compartment baseplate for the model FTIR instrument you specified. Before inserting the accessory in the sample compartment, ensure that your spectrometer is aligned. If the instrument is not aligned, maximize the interferogram signal (the IR energy throughput) of your FTIR spectrometer. This should be performed by following the manufacturer’s instructions.

3. Fasten the accessory directly into the FTIR sample compartment or onto the FTIR sample

compartment baseplate using the 2 screws located one on each side of the GladiATR Vision base optics (Figure 1). In order to locate the accessory in the correct position, simply place the entire accessory into the FTIR sample compartment with the GladiATR Vision label facing the front and line up the baseplate provided with the holes/pins in your model FTIR spectrometer.

4. Tighten the mounting screws to firmly position the accessory baseplate onto the FTIR sample

compartment baseplate. 5. Mount the pressure clamp onto the back side of the accessory using the two alignment dowel pins

on top of the GladiATR Vision base and fasten using the two hex-head screws into the clamp frame. 6. Install the IC 2.2 software and cables for the BNC version of the GladiATR Vision or Videology

software for the USB configuration. Follow instructions in the next section for your specific accessory model.

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Software Installation The GladiATR Vision may be configured for either a USB bus, most often, or a BNC connector. If you have the USB bus, follow the Installing Videology Image Capture Software instructions. For the BNC connector, follow the Installing IC 2.2 Image Capturing Software instructions.

Installing Videology Image Capture Software (USB) Minimum system requirements for the Videology software are a PC with a USB 2.0 compatible port, Windows XP (service pack 2 preferred) or Windows 7, Pentium 4 2.0 GHz, hard drive speed 5,400 RPM, and 128 MB of RAM. Videology CD will automatically launch the installation wizard. If this does not occur, select autorun.exe file located on the software CD. Be sure the USB cable is NOT connected to the computer USB port at this time. You will be prompted to connect the USB cable from the Vision to the computer USB port during installation. After the USB connection wait a few moments for your computer to recognize the hardware. Additional installation information is located in the Videology manual found on the Videology CD.

Interfacing with the GladiATR Vision 1. With the LCD screen powered on, open the Videology Viewer software. The camera image should be

shown on the computer screen. If the image is not shown, select Advanced Option found under the Options drop down menu. Check Isochronous Pipe, which determines how the streaming video is sent through the USB bus. Under the Options drop down menu, select camera settings. The Video Capture Filter Properties should be set to CVBS as the source and NTSC_M as the format.

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2. Prior to capturing images set the folder where images will be saved. From the file menu, select Set Snap Image Folder and assign a folder. An image is saved by selecting Take Snapshot in the File menu.

The GladiATR Vision is now ready for alignment.

Installing IC 2.2 Image Capturing Software (BNC) IC 2.2 is an optional component for the GladiATR Vision that allows the LCD image to be captured and saved as a .jpg file. To capture saved images, the computer requirements are PC or laptop with PIII/800 MHz/256 MB or higher, a USB 2.2 interface, and Windows XP/SP2, Windows Vista (32 or 64 bit), or Windows 7 as the operating system. 1. Prior to installing the software, connect the BNC-to-composite video cable to the BNC jack located

on the front of the GladiATR Vision and to the Imaging Source box. Also, connect the USB cable to the USB 2.0 on the computer and to the Imaging Source box. Then, power up the LCD screen.

2. Follow the Getting Started instructions provided by Image Sourcing for the Video-to-USB Converter DFG/USB2-It.

3. With the LCD screen powered on, open the IC 2.2 software. Select the DFG/USB2-It drive. The following settings should be shown on the device bar. With the exception of the FPS (frames per second), which is a default value depending on the configuration of the computer, the settings should mimic those shown below - make sure NTSC_M is selected.

4. The LCD image transferred to the computer screen is live. If the image is a still frame, go to the device menu and select “live” (or press ctrl-l). Image color saturation, brightness, contrast, and sharpness may be tuned to preference through “properties” found in the device drop-down menu.

5. Images are easily saved by selecting “save image” in the drop-down “capture” menu in either .jpg or .bmp format. The snap image option in the capture menu will cause the image on the computer to become still framed; the image on the GladiATR Vision screen remains live. To return to a live image on the computer screen, select “live” in the device menu or press ctrl-l.

The GladiATR Vision accessory is now ready for optical alignment.

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Accessory Alignment

The GladiATR Vision accessory may not require any alignment when installed - see page 12 for minimum values. However, should you choose to fine-tune the accessory, follow these steps: 1. Make sure the LCD display is turned off and the power input is removed. Remove the front panel of

the GladiATR Vision accessory by loosening the 4 hex head retaining screws, two on each side of the front panel. Pull the front panel forward to release from the screws and place it in a secure resting place on top of the crystal plate on top of the GladiATR Vision base optics (position the High- Pressure Clamp in the back rotated position to make room for the front panel). Do not undo the electrical wires connecting the camera and the front panel.

2. Display the live interferogram of the FTIR spectrometer and adjust the input optic, the crystal focus

and the relay mirror. To do this, turn the individual screws one at a time slightly clockwise and check the signal. If it increases, continue until the maximum signal is obtained. If it decreases, turn the screw counterclockwise to get the highest possible reading. Follow the order shown in the alignment image, first adjusting the input optic screw to obtain the maximum signal, then go to the 2 sets of crystal focus screws and optimize the interferogram signal.

Figure 6. Alignment of the GladiATR Vision

Input Optics

Crystal Focus

Relay Mirror

Do not adjust

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3. Finally, adjust the relay mirror screws to optimize the interferogram signal.

4. Repeat the entire procedure 2-3 times to fine-tune the accessory. This is an initial (one-time) alignment procedure which optimizes the GladiATR Vision to work with an individual optical bench. Once completed, the alignment does not have to be repeated, unless the accessory adjustments have been moved or it has been placed in a different FTIR instrument.

You are now ready to verify the GladiATR Vision optical throughput performance.

Adjusting Camera Focus

The camera was focused prior to leaving our facility. You may choose to adjust as clamp pressure may affect the focusing distance causing a less sharp image. To adjust the camera focus, loosen four hex screws located on the sides of the front panel, which secure the front accessory panel with the LCD screen. Remove the front panel to access the focusing thumb wheel. To adjust the camera focus, loosen the button head screw located underneath the focus thumb wheel. Monitor the image quality while turning the thumb wheel to the left and right. Only small left or right movements should be required. Once the optimal focus has been found, tighten the button head screw and secure the front panel with the 4 hex screws located on the front panel sides.

Figure 7. Camera focus adjustment

Camera Focus Adjustment Thumb-Wheel Button Head Screw

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Performance Verification

1. With the accessory removed from the sample compartment, collect an open beam background spectrum.

2. Place the aligned GladiATR Vision accessory into the instrument. 3. Collect a transmission spectrum using the same collection parameters as used to collect the

background spectrum. This resulting spectrum is termed a throughput spectrum and measures the IR spectrum of the GladiATR Vision accessory.

4. Place a cursor on the throughput spectrum at 1000 cm-1 and record the value in % transmission.

NOTE: Each of the different crystals (diamond or Ge) will have different looking spectra. An example throughput spectrum for diamond is shown below. Diamond has strong, broad phonon absorbance bands in the region of 2100 cm-1. This is normal and will ratio out well in resulting spectra.

The following are the % transmission values the accessory should achieve with different crystal configurations at 1000 cm-1.

Diamond Crystal Plate: Greater than 14%T Ge Crystal Plate: Greater than 14%T

GladiATR Throughput

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If your accessory does not meet this minimum transmission level, please contact PIKE Technologies. Before making this call, please record the serial number located on the label on the back of the GladiATR Vision base optics assembly.

NOTE: IR throughput performance of your accessory may decrease slowly over time as the ATR crystal plate surface is exposed to normal wear from cleaning the ATR surface. Please Contact PIKE Technologies for information about GladiATR Vision service when transmission throughput drops below a usable level.

Sampling Procedures

Collect the background spectrum with the accessory in the sample compartment. Make sure the ATR crystal is clean and free of any residues. Once completed, place the sample on the crystal surface (apply the clamp if solid) and collect sample spectrum. A single crystal plate design is used for all types of samples (liquids, pastes, powders, soft pliable films and solids).

The sample must be in intimate contact with the ATR crystal surface for the evanescent wave to provide an ATR signal. Note that the Ge crystal used in the accessory is made of materials considerably softer than diamond. Ge can be scratched if care is not used to remove samples. Scratches on the surface of the crystal will result in a reduction in the throughput of the accessory. Remove the sample gently with a non-abrasive cotton tissue and clean with solvent. The crystal plate should be cleaned with an appropriate mild solvent, such as isopropyl alcohol or a stronger solvent, such as acetone. Cotton swabs are highly recommended for ease of cleaning without scratching the ATR crystal surface.

Sometimes “carry over” may occur from one sample to another due to incomplete cleaning of a prior sample from the face of the crystal. This effect may be minimized by collecting a new background spectrum before each sample spectrum.

Samples should not be left in contact with the crystal for an extended period of time since some samples may degrade the crystal material and discoloration of the metal plate can occur. Once the measurement has been made, remove the sample from the crystal and clean the surface of the crystal and the surrounding plate area with a suitable solvent. Note that the High-Pressure Clamp for the GladiATR can be swung back to give more access to the ATR crystal area by loosening the smaller clamp knob.

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Sample Analysis with High-Pressure Clamp 1. Loosen the small, arm-securing knob.

2. Raise the clamp arm up and place your sample on the diamond crystal. Some friction during the arm movement is normal as it prevents its accidental drop and crystal damage.

3. Lower the arm, slightly push the arm-securing knob down and tighten it all the way (please do not use any tools in this process as finger pressure alone is sufficient).

4. Turn the large clamp knob clockwise to compress the sample. Two “clicks” indicate that the optimum pressure has been achieved.

5. After the measurement is completed, release the main knob first and the small knob second if the arm needs to be raised. Please keep in mind that the small knob is spring loaded and it needs to be pressed in for the screw to engage again.

CAUTION: GladiATR crystal damaged by excessive pressure cannot be covered by the warranty. Caution is required when using the High-Pressure Clamps with the Ge ATR plate. The diamond crystal plate is very rugged. This crystal will withstand higher pressures than traditional IR materials, but it still may be damaged by an excessive force. For this reason, do not exceed the pressure originally set by the factory on the High-Pressure Clamps. The applied pressure is a function of the size of the pressure tip for large samples or the size of the sample for small samples.

Main pressure tower knob

Small, arm-securing knob

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Pressure Clamp Tip Attachments The success of an ATR measurement depends upon the quality of the contact between the sample and the crystal. Since there is an infinite number of sample shapes and types, a single configuration of the sample press tip may not be adequate. For this reason, the GladiATR pressure clamp is designed to accept three different tip attachments, providing the best possible configuration for any given sample type.

The accessory is shipped with the swivel tip attached to the pressure clamp ordered with the GladiATR accessory. This tip features an end cap mounted onto a small ball joint. Such design allows the pressure tip to move and adjust its position to the shape of the sample and maintain the sample position parallel to the crystal surface. This tip allows for better positioning and optimal contact of thin materials with the ATR crystal surface. The swivel tip is used with irregularly shaped samples, films, semi-rigid polymers (e.g. credit card like materials).

The flat tip attachment is a flat-tipped cone and it is used when analyzing thin films, fibers, small particles, rubber samples and other elastic polymers. The flat tip may also be used for powdered samples.

The concave tip was developed specifically to work with granules, large beads and polymer pellets. The tip features a concaved surface which prevents the sample from escaping from underneath the press. It also forces the spherical samples to stay in the center of the crystal, assuring maximum IR signal strength. Do not use the concave tip for powdered samples or samples which do not completely protect the concave edges of the steel tip from pressing against the ATR crystal - this will damage the ATR crystal.

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Configuration for Liquid Sampling

The crystal plate assembly of the GladiATR accessory features a round plate design with a 3.0 mm diameter ATR crystal sampling area located in the center of the plate. For liquid sampling, a droplet of the sample is placed onto the ATR crystal.

For volatile liquids, the optional Liquids Retainer with Volatiles Cover reduces the amount of evaporation of the sample on the surface of the crystal. To use, place the retainer disk over the ATR crystal. Place the U-shaped bridge over the retainer disk. Apply pressure to the U-shaped bridge using the pressure clamp. Fill the reservoir of the Liquids Retainer with the volatile liquid. Slide the Volatiles Cover between the retainer disk and the U-shaped bridge (Figure 10).

Figure 10. Proper placement of a Liquids Retainer and Volatiles Cover on the GladiATR accessory

For continuous sample monitoring, or for applications where the sample needs to be completely enclosed for safety or reactivity reasons, an optional Flow-Through Attachment is available. To use, place the Flow-Through Attachment over the ATR crystal. Apply the clamp to the top of the Flow-Through Attachment, which creates a seal between the O-ring located on the underneath side of the Flow-Through Attachment and the ATR crystal plate (Figure 11). Using the Luer-Loc fitting, load the sample by connecting a syringe or a flow line.

Volatiles Cover

Liquids Retainer

U-Shaped Bridge

Figure 11. GladiATR with Flow-Through Attachment

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One minute, 4 cm-1 resolution spectra of a dilute detergent solution and distilled water were collected using the GladiATR Vision with diamond crystal. These samples were applied directly onto the GladiATR diamond ATR crystal for analysis.

The red spectrum is the detergent solution and the blue spectrum is that for distilled water. A spectral subtraction can be applied to obtain the spectrum of the detergent component. This is shown in the red spectrum on the right, and the result will represent the detergent contribution of the liquid sample.

Detergent Solution Distilled H20

Subtraction Result; Detergent Solution

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Configuration for Solid Sampling For measurements of soft pliable films and selected solid samples, the sample is placed onto the surface of the crystal. Since the ATR effect only takes place very close to the surface of the crystal, an intimate contact has to be made by the sample on the ATR crystal surface. This is achieved by using the pressure clamp ordered with your GladiATR system. With the sample in place on the crystal, lower the pressure tip so that it is in contact with the sample. You can continue to turn the pressure knob and increase pressure to a desired level to obtain a spectrum. However, in most cases, it is recommended to apply the maximum pressure allowed to ensure the best contact and highest sampling sensitivity. The force applied by the High-Pressure Clamps is factory set to 40 pounds. The applied pressure is then a function of the size of the pressure tip for large samples or the size of the sample for small samples. For example, 40 pounds of force upon a sample which completely covers the crystal will generate 6,789 psi whereas 40 pounds of force upon a 1.0 mm diameter flat sample will generate 32,858 psi. The High-Pressure Clamp has a slip clutch mechanism to avoid exceeding 40 pounds of force. CAUTION: Care must be used in operating the pressure clamps, since for small hard samples the maximum pressure may be exceeded. For the analysis of solid samples the pressure clamp of the GladiATR is required. The sample is placed face down onto the diamond crystal and force is applied to make intimate contact onto the ATR crystal. The GladiATR accessory enables us to position the sample to a feature area to ensure that the spectrum collected is taken from the desired location on the sample. The spectrum below is collected from the print area on paper. For this analysis pressure was applied to the sample using the swivel tip. The acquisition time was one minute and the spectral resolution was set to four wavenumber.

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Configuration for Powder Sampling

Most powders may be analyzed with an ATR accessory. Note that since the ATR effect requires the sample to be in intimate contact with the crystal, this method is most effective when analyzing soft powders.

Crystal Cleaning The solvent used for cleaning your crystal is dependent on the sample that has been analyzed. In all cases it is best to attempt to clean the crystal with the mildest solvent possible. For most cases, the preferred solvent is isopropyl alcohol. If a stronger solvent is required, acetone may be used. In very stubborn cases dimethylformamide may be used. In all cases when using solvents, inspect the materials safety data sheet associated with the solvent you are using and comply with any recommended handling procedures. Apply the solvent to the crystal with a cotton swab and gently remove using the cotton swab or non-abrasive wipe. Repeat this procedure until all traces of the sample have been removed. Under no circumstances should the softer crystal materials (Ge) be rubbed with paper products such as “Kleenex” or “Kim wipes”. Many paper products are abrasive and could cause scratching of the softer crystal surfaces.

Effects of Temperature The PIKE Technologies GladiATR Vision utilizes brazing and bonding technology to seal the crystal to its mount. This sealing mechanism allows some flexibility and hot samples may be placed on the crystal without damaging the crystal or seal. However, it is recommended that the temperature difference between the sample and the crystal be not more than 30 °C.

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ATR Spectra

ATR spectra are similar to transmission spectra. A careful comparison of ATR spectra and transmission spectra reveals that the intensities of the spectral features in an ATR spectrum are of lower absorbance than the corresponding features in a transmission spectrum and especially in the high wavenumber (short wavelength) region of the spectrum. The intensity of the ATR spectrum is related to the penetration depth of the evanescent wave into the sample. This depth is dependent on the refractive index of the crystal and the sample, and upon the wavelength of the IR radiation.

The relatively thin depth of penetration of the IR beam into the sample creates the main benefit of ATR sampling. This is in contrast to traditional FT-IR sampling by transmission where the sample must be diluted with IR transparent salt, pressed into a pellet or pressed to a thin film, prior to analysis to prevent totally absorbing IR bands.

A comparison of transmission vs. ATR sampling result for a thick polymer sample is shown below where the sample is too thick for high quality transmission analysis (shown in the lower spectrum). In transmission spectroscopy, the IR beam passes through the sample and the effective pathlength is determined by the thickness of the sample and its orientation to the directional plane of the IR beam. Clearly in the example shown below the sample is too thick for transmission analysis because most of the IR bands are totally absorbing.

However, simply placing the thick sample on the ATR crystal and applying pressure generates a high quality spectral result (upper red spectrum) - identified by library search as a polybutylene terephthalate. The total analysis time for the thick polymer by ATR was less than one minute.

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ATR Correction

If an ATR spectrum representative of a transmission spectrum is desired, the ATR spectrum must be processed with the ATR correction program available in your instrument software. An example of the effect of this correction on a spectrum is shown in the following example for polystyrene. The middle spectrum is the original ATR spectrum of polystyrene. The lower spectrum is the transmission spectrum of polystyrene. Clearly the IR bands around 3000 cm-1 in the ATR spectrum are weaker relative to the IR bands at longer wavelength.

However, in the upper red spectrum after ATR correction, the relative IR band intensities are very similar to those from the polystyrene run by transmission.

Polystyrene, ATR Corrected

Polystyrene, ATR, Original Spectrum

Polystyrene, 1.5 mil. film, by transmission

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Useful Equations

The depth of penetration gives us a relative measure of the intensity of the resulting spectrum and is expressed by the following equation:

𝑑𝑝 =𝜆

2𝜋( 𝑛12 𝑠𝑠𝑛2 θ − 𝑛22 )1/2

Where λ is the wavelength of light, n1 is the refractive index of the crystal, n2 is the refractive index of the sample and θ is the effective angle of incidence. Depth of penetration in microns as a function of crystal material is shown in the table below. The penetration depth is calculated for a sample with a refractive index of 1.5 at 1000 cm-1.

Crystal ATR Materials

Material RI dp (µ) @1000 cm-1 pH Range Long Wave Cutoff

Diamond 2.4 2.0 1-14 10 cm-1

Ge 4.0 0.66 1-14 450 cm-1

Diamond

Diamond is one of the most rugged optical materials. It can be used for analysis of a wide range of samples, including acids, bases, and oxidizing agents. Diamond is also scratch and abrasion resistant. Its disadvantage is the intrinsic absorption from approximately 2300 to 1800 cm-1 which limits its usefulness in this region for detecting extremely small absorbance across this spectral range.

Germanium Germanium has been used extensively in the past as a higher refractive index material for samples that produce strong absorptions such as rubber O-rings. The crystal is also used when analyzing samples that have a high refractive index, such as in passivation studies on silicon.

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Precautions

Mirrors

In order to provide the maximum reflectivity in the infrared, with the minimum spectral interferences, the mirrors used in this device are uncoated (bare) aluminum. Normally, these mirrors will not require cleaning, since they are contained within the housing of the accessory. If they do need cleaning, please contact PIKE for recommendations. Under no circumstances must the mirrors be rubbed with paper products since this will produce scratching of the mirror surface.

SAFETY

Caution should be used when handling and using ATR crystals since some of the materials can be hazardous. If the crystal is broken or pulverized, the dust may be harmful by inhalation, ingestion or skin absorption.

Protection provided by the equipment may be impaired if the equipment is used with accessories not provided or recommended by the manufacturer, or is used in a manner not specified by the manufacturer.

Periodically inspect the External Power Supply interconnect cord and other parts for damage. If any damage is observed, do not use the equipment and contact PIKE Technologies for replacement parts.

Do not position the equipment in a space where it is difficult to disconnect the power cord at the front of the equipment.

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Environmental Ratings

Installation Category II (Transient over-voltage)

Pollution Degree 2 (Temporary conductivity caused by condensation)

Altitude Limit 2,000 meters

Use “Indoor” use

Ambient Temperature 40 °C max

Humidity 80 % RH non-condensing

Specifications

ATR Crystal Choices Diamond, germanium (non-viewing)

Crystal Plate Mounting User changeable plates

Crystal Type Monolithic

Diamond set Brazed

Crystal Plate Mounts Stainless steel

Angle of Incidence 45°, nominal

Crystal Dimensions, Surface 3.0 mm diameter

Optics All reflective

Pressure Device Rotating, continuously variable pressure; click stop at maximum

Maximum Pressure 30,000 psi

Sample Access 80 mm, ATR crystal to pressure mount

Spectral Range, Diamond 4000 to 10 cm-1 (IR optics dependent)

Viewing Option Integrated 4” LCD Magnification 110X magnification

View Area 770 x 590 microns

Optional Image Save USB image capture

Viewing Mode Through diamond crystal

Input Voltage 90-264 V, auto setting, external power supply

Operating Voltage 12 VDC Wattage 18 watts max

External Power Supply 100-240 VAC, 50/60 Hz, 0.6 Amps max.

Specular Reflection Option Optional, 45° nominal angle of incidence

Purge Purge tubes and purge line connector included Accessory Dimensions

(W x D x H) 140 x 225 x 340 mm (excludes FTIR baseplate and mount)

FTIR Compatibility Most, specify model and type

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Power Supply Symbol Definitions

DC - Direct Current

AC - Alternating Current

Equipment protected throughout by Double or Reinforced Insulation

Label Description Location

CE marking indicates the accessory complies with the essential requirements of the relevant European health, safety and environmental protection legislations.

This symbol is located on the backside of the GladiATR Vision.

The RoHS symbol indicates this product is free from RoHS prohibited elements and compounds (Pb, Cd, Hg, Hex-Cr, PBB, and PBDE).

This symbol is located on the backside of the GladiATR Vision.

The crossed out wheeled bin is a clear reminder that the product must not be disposed with household waste. It is the responsibility of the buyer to discard the product in accordance with federal, regional, and local environmental regulations.

This symbol is located on the backside of the GladiATR Vision.

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Replacement Parts and Options

The following parts and options may be ordered for the GladiATR Vision accessory:

GladiATR Vision Crystal Plates

Part Number Description 026-2102 Diamond Vision Crystal Plate 026-2050 Ge Crystal Plate (non-viewing) 026-2200 Specular Reflection Plate (non-viewing) 026-4101 Heated Diamond Crystal Plate, 210 °C, Vision 026-4050 Heated Ge Crystal Plate, 130 °C (non-viewing)

GladiATR Vision Image Capture Option

Part Number Description 026-3510 USB Interface Adapter and Software for BNC model of GladiATR Vision

Temperature Controllers

Part Number Description 076-1220 Digital Temperature Control Module (210 °C) 076-1420 Digital Temperature Control Module, PC Control (210 °C)

Pressure Clamp

Part Number Description 026-3020 High-Pressure Clamp 076-6026 Digital Force Adapter for High-Pressure Clamp

Other Attachments

Part Number Description 026-5012 Flow-Through Attachment 026-5013 Liquids Retainer and Volatiles Cover Set 026-5010 Liquids Retainer for Performance Plates 026-3051 Volatiles Cover for Performance Plates 025-3095 Flat Tip 025-3093 Swivel Tip 025-3092 Concave Tip

6125 Cottonwood Drive · Madison, WI 53719-5120 · (608) 274-2721 (TEL) · (608) 274-0103 (FAX) info@piketech.com · www.piketech.com